WO2015007450A1 - Method for filling cavities in hollow bricks with a thermal insulation material mixture containing a hydrophobing agent - Google Patents

Method for filling cavities in hollow bricks with a thermal insulation material mixture containing a hydrophobing agent Download PDF

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Publication number
WO2015007450A1
WO2015007450A1 PCT/EP2014/062816 EP2014062816W WO2015007450A1 WO 2015007450 A1 WO2015007450 A1 WO 2015007450A1 EP 2014062816 W EP2014062816 W EP 2014062816W WO 2015007450 A1 WO2015007450 A1 WO 2015007450A1
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WO
WIPO (PCT)
Prior art keywords
mixture
filling tube
weight
hollow chambers
process according
Prior art date
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PCT/EP2014/062816
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German (de)
French (fr)
Inventor
Günter Kratel
Thomas Eyhorn
Original Assignee
Evonik Industries Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Evonik Industries Ag filed Critical Evonik Industries Ag
Priority to EP14731266.4A priority Critical patent/EP3022025B1/en
Priority to PL14731266T priority patent/PL3022025T3/en
Publication of WO2015007450A1 publication Critical patent/WO2015007450A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00—Compositions for artificial stone, not containing binders
    • C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/04—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers
    • B28B11/042—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers with insulating material
    • B28B11/043—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers with insulating material filling cavities or chambers of hollow blocks
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04C—STRUCTURAL ELEMENTS; BUILDING MATERIALS
    • E04C1/00—Building elements of block or other shape for the construction of parts of buildings
    • E04C1/40—Building elements of block or other shape for the construction of parts of buildings built-up from parts of different materials, e.g. composed of layers of different materials or stones with filling material or with insulating inserts
    • E04C1/41—Building elements of block or other shape for the construction of parts of buildings built-up from parts of different materials, e.g. composed of layers of different materials or stones with filling material or with insulating inserts composed of insulating material and load-bearing concrete, stone or stone-like material

Definitions

  • the invention relates to a method for filling the hollow chambers of
  • Styrofoam foam or perlite foam to fill.
  • the filled perforated bricks obtained in this way have an improved thermal insulation capacity compared with the unfilled perforated bricks.
  • a disadvantage is the declining thermal insulation by the inclusion of
  • EP-A-1988228 a process is disclosed in which an insulating material containing pyrogenic silica, opacifiers and fibers and a hydrophobing agent is compressed into dimensionally accurate plates and incorporated in the Cavities used the hollow brick.
  • the procedure is similar in DE-A-10 2009 054 566 and DE-A-10 2010 029 513.
  • DE-A-10 2010 029 513 proposed to fill the admixed with the hydrophobing agent mixture in the hollow chambers of perforated bricks and to press by means of pressing aids directly into the hollow chambers.
  • the admixed with the hydrophobing agent mixture can be insufficiently compressed.
  • the invention relates to a method for filling the hollow chambers of perforated bricks with a thermal insulation mixture, in which
  • Hydrophobizing agent promotes into an upper filling tube (2)
  • Hydrophobing agent and the completion of the pressing process does not exceed 60 minutes and
  • the numbering (1) - (7) relates to FIG. 1.
  • A means the movement of the ram (5) down
  • B the two-sided pressing of the ram (5) and (6).
  • Silicon compounds such as chlorosilanes produced.
  • a hydrolyzable silicon halide is reacted with a flame formed by combustion of hydrogen and a
  • a silica prepared in this way is called fumed silica. In this process, first Primary particles formed that are almost free of internal pores.
  • fumed silica is an ideal insulating material because of its structure
  • the fumed silica used is a hydrophilic silica, as used in the US Pat
  • This silica carries on its
  • the silanol group density is generally from 1.8 to 2.5 when obtained by reaction of the silica powder with LiAlH 4 according to the method of J. Mathias and G. Wannemacher (Journal of Colloid and Interface Science 125, 1988, 61) is determined.
  • the surface of the hydrophilic silica should not be treated with an organic or inorganic hydrophobing agent.
  • fumed silica means a powdery, fumed, hydrophilic silica.
  • the fumed silica can also be in a condensed form, ie with
  • the opacifiers used in the process according to the invention are preferably titanium oxides, zirconium oxides, ilmenites, iron titanates, iron oxides, zirconium silicates, silicon carbide, manganese oxides, graphites and / or carbon blacks, or mixtures of substances which comprise at least one of the abovementioned constituents. Particular preference is given to silicon carbide, titanium oxides, iron oxides or carbon blacks.
  • the particle size of the opacifier is usually between 0.1 to 25 ⁇ . In the case of silicon carbide and titanium oxides, the mean particle diameter d 5 o is preferably 1 to 10 ⁇ m, more preferably 2 to 8 ⁇ m.
  • fibers may be of inorganic or organic origin.
  • examples of usable inorganic fibers are glass wool, rock wool, basalt fibers, slag wool and ceramic fibers, which consist of melts of alumina and / or silica, and other inorganic metal oxides.
  • Pure silica fibers are, for example, silica fibers.
  • usable organic fibers are cellulose fibers, textile fibers or
  • the diameter of the fibers is preferably 1 to 30 ⁇ , more preferably 5 to 15 ⁇ , most preferably 6 to 9 ⁇ , and the length is preferably 1 to 25 mm, more preferably 3 to 12 mm.
  • Hydrophobizing agent is preferably 0.5 to 10 wt.%, Particularly preferably 1 to 6 wt.%, Each based on the mixture (1).
  • the hydrophobing agent is introduced in liquid form, as finely divided as possible into the mixture (1).
  • the mixture (1) is preferably in motion, for example by stirring.
  • the hydrophobizing agent can be introduced by a compressed air-free atomization or by in the mixture (1) projecting cannulas.
  • this process is carried out in a period of not more than 5 minutes, more preferably from 10 seconds to 3 minutes and most preferably from 30 seconds to 90 seconds.
  • the process step of the hydrophobing is dependent on the water content of the fumed silica.
  • the water content should not be more than 1% by weight, based on the mixture (1).
  • perforated bricks and cold-formed bricks for example cement-bound pumice stones, can be used as perforated bricks (4).
  • the process according to the invention has a reaction step in which the compressed mixture in the hollow chambers of the perforated brick (4) can be allowed to react.
  • the secondary reaction essentially serves to hydrophobize
  • Reaction to be carried out so that, starting from 20-30 ° C continuously heated over a period of 20-90 minutes, more preferably 30-60 minutes to a temperature of 50-100 ° C, and optionally at the highest
  • the compressed mixture can sometimes have a so-called "spring-back" effect, that is, it can expand slightly after pressing, which on the one hand leads to the necessary anchoring in the hollow chamber of the building block, on the other hand, a part of the compressed mixture on the
  • Hollow brick MZ 8 with 12 hollow chambers, brick composite "My brick house”.
  • Mixture (1) A mixture consisting of 83% by weight of AEROSIL® 200, Evonik, 16% by weight of silicon carbide and 1% by weight of fibers is used.
  • the hydrophobizing agent used is hexamethyldisilazane, 4% by weight, based on the mixture (1).
  • the mixing operation is carried out in a closed container using a stirrer at a rotation speed of 1000 - 1500 rpm.
  • the stirring time is approx. 30 - 60 s, during which time the water repellent is injected for the first 30 - 45 s and then stirred for a further 15 s.
  • the temperature is about 20 ° C on.
  • the mixture is conveyed into the upper filling tube (2).
  • the lower ram (5) moves downwards (A) and sucks the mixture through the hollow chamber of the perforated brick (4) into the lower filling tube (3).
  • the compaction of the mixture takes place during pressing at the same time and on both sides 2 - 3 mm into the perforated brick.
  • the excess air is sucked through filter plates through the press punches (7).
  • the pressing process is completed within 10 minutes. Subsequently, the temperature is increased to 60 ° C over a period of 50 min and left there for 10 min. After about 30 - 45 minutes at a temperature of about 60 ° C is the Completed reaction in the perforated brick, the thermal insulation mixture continuously hydrophobic and the degassing occurs largely.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Silicon Compounds (AREA)
  • Thermal Insulation (AREA)

Abstract

The invention relates to a method for filling cavities in hollow bricks with a thermal insulation material mixture, according to which method: a) a mixture (1), which is obtained by adding a liquid hydrophobing agent to a pulverulent, pyrogenic, hydrophilic silicic acid, pulverulent opacifier and fibres at temperatures of less than 30°C, is conveyed into an upper filling tube (2); b) the lower plunger (5) is then moved downwards and thus some of the mixture in the upper filling tube (2) is sucked through the cavities in the hollow brick (4) into the lower filling tube (3), such that the mixture is distributed into the upper filling tube (2), the cavities in the hollow brick (4) and the lower filling tube (3); c) the mixture is then compressed by pressing the plungers (5) and (6) on both sides; d) wherein gaseous and possibly vaporous substances are removed before and during the pressing process via filter plates (7) on the plungers (5) and (6); e) wherein the period between the addition of the liquid hydrophobing agent and the conclusion of the pressing process does not exceed 60 minutes; and f) the mixture that has been compressed in the cavities in the hollow brick (4) is then allowed to react, preferably at a temperature of 20 to 100°C.

Description

Verfahren zur Befüllung der Hohlkammern von Lochziegeln mit einer ein Hydrophobierungsmittel enthaltenden Wärmedämmstoffmischung  Method for filling the hollow chambers of perforated bricks with a thermal insulation mixture containing a hydrophobizing agent
Die Erfindung betrifft ein Verfahren zur Befüllung der Hohlkammern von The invention relates to a method for filling the hollow chambers of
Lochziegeln mit einer ein Hydrophobierungsmittel enthaltenden Hollow bricks with a hydrophobizing agent
Wärmedämmstoffmischung. Thermal insulation material mixture.
Es ist bekannt die Hohlkammern von Lochziegeln Dämmmaterialien wie It is well known the hollow chambers of perforated bricks insulation materials
Styroporschaum oder Perlite-Schaum zu füllen. Dabei bringt man in der Regel Schüttungen in die Hohlkammern ein und schäumt anschließend mittels Styrofoam foam or perlite foam to fill. In this case, one usually brings in beds in the hollow chambers and then foams by means
Wasserdampf auf. Die so erhaltenen gefüllten Lochziegel weisen eine gegenüber den ungefüllten Lochziegeln verbesserte Wärmedämmfähigkeit aus. Als nachteilig hat sich die nachlassende Wärmedämmfähigkeit durch die Aufnahme von Water vapor on. The filled perforated bricks obtained in this way have an improved thermal insulation capacity compared with the unfilled perforated bricks. A disadvantage is the declining thermal insulation by the inclusion of
Feuchtigkeit und/oder die Brennbarkeit der Dämmmaterialien erwiesen. Moisture and / or the combustibility of the insulating materials proved.
Dies Nachteile können weitestgehend vermieden und die Wärmedämmfähigkeit verbessert werden, indem man Dämmmaterialien einsetzt, die pyrogene These disadvantages can be largely avoided and the thermal insulation ability can be improved by using insulating materials, the pyrogenic
Kieselsäure enthalten und die hydrophobe Eigenschaften aufweisen. Contain silica and have the hydrophobic properties.
So ist in EP-A-2028329 ein Verfahren beschrieben, bei dem das pyrogene Kieselsäure enthaltende Dämmmaterial als Schüttgut mit einer sackartigen Umhüllung in die Hohlräume eingebracht wird. Thus, in EP-A-2028329 a method is described in which the fumed silica-containing insulating material is introduced as bulk material with a bag-like envelope in the cavities.
In EP-A-1988228 ist ein Verfahren offenbart, bei dem man ein Dämmmaterial, welches pyrogen hergestellte Kieselsäure, Trübungsmittel und Fasern und ein Hydrophobierungsmittel enthält zu maßgenauen Platten verpresst und diese in die Hohlräume der Hochlochziegel einsetzt. Analog wird in DE-A-10 2009 054 566 und DE-A-10 2010 029 513 vorgegangen. In EP-A-1988228 a process is disclosed in which an insulating material containing pyrogenic silica, opacifiers and fibers and a hydrophobing agent is compressed into dimensionally accurate plates and incorporated in the Cavities used the hollow brick. The procedure is similar in DE-A-10 2009 054 566 and DE-A-10 2010 029 513.
Die genannten Verfahren sind aufgrund der bei Hochlochziegel vorliegenden Maßtoleranzen nur sehr aufwändig durchzuführen. Because of the dimensional tolerances present in hollow bricks, the abovementioned methods can only be carried out with great difficulty.
Als Alternative wird in EP-A-1988228, DE-A-10 2009 054 566 und As an alternative, in EP-A-1988228, DE-A-10 2009 054 566 and
DE-A-10 2010 029 513 vorgeschlagen, die mit dem Hydrophobierungsmittel versetzte Mischung in die Hohlkammern der Hochlochziegel einzufüllen und mittels Presshilfen direkt in den Hohlkammern zu verpressen. Es wurde jedoch gefunden, dass sich die mit dem Hydrophobierungsmittel versetzte Mischung nur unzureichend verpressen läßt. DE-A-10 2010 029 513 proposed to fill the admixed with the hydrophobing agent mixture in the hollow chambers of perforated bricks and to press by means of pressing aids directly into the hollow chambers. However, it has been found that the admixed with the hydrophobing agent mixture can be insufficiently compressed.
Es bestand daher die technische Aufgabe ein Verfahren bereitzustellen, welches das Verpressen eines eine pyrogene Kieselsäure enthaltenden Dämmmaterials in den Hohlkammern eines Hochlochziegels zuläßt. It was therefore the technical problem to provide a method which allows the compression of a pyrogenic silica-containing insulating material in the hollow chambers of a perforated brick.
Gegenstand der Erfindung ist ein Verfahren zur Befüllung der Hohlkammern von Lochziegeln mit einer Wärmedämmstoffmischung, bei dem man The invention relates to a method for filling the hollow chambers of perforated bricks with a thermal insulation mixture, in which
a) ein Gemisch (1 ) das erhalten wird, indem man eine pulverförmige, pyrogene, hydrophile Kieselsäure, pulverförmiges Trübungsmittel und Fasern, bei Temperaturen von weniger als 30 °C mit einem flüssigen a) a mixture (1) which is obtained by reacting a powdered, fumed, hydrophilic silica, powdered opacifier and fibers, at temperatures of less than 30 ° C with a liquid
Hydrophobierungsmittel versetzt, in eine obere Füllröhre (2) fördert,  Hydrophobizing agent, promotes into an upper filling tube (2),
b) nachfolgend den unteren Pressstempel (5) nach unten bewegt und so einen Teil der sich in der oberen Füllröhre (2) befindlichen Mischung durch die Hohlkammern des Lochziegels (4) in die untere Füllröhre (3) saugt, so dass sich die Mischung in die obere Füllröhre (2), die Hohlkammern des Lochziegels (4) und in die untere Füllröhre (3) verteilt, b) subsequently moves the lower ram (5) downwards and thus sucks a part of the mixture located in the upper filling tube (2) through the hollow chambers of the perforated brick (4) into the lower filling tube (3), so that the mixture is distributed in the upper filling tube (2), the hollow chambers of the perforated brick (4) and in the lower filling tube (3),
c) nachfolgend durch beidseitiges Pressen der Pressstempel (5) und (6) die c) subsequently by pressing both sides of the ram (5) and (6) the
Mischung verdichtet,  Compacted mixture,
d) wobei vor und während des Pressvorganges gasförmige und gegebenenfalls dampfförmige Stoffe über Filterplatten (7) an den Pressstempeln (5) und (6) entfernt wird und d) wherein before and during the pressing process gaseous and optionally vaporous substances on filter plates (7) on the press dies (5) and (6) is removed and
e) wobei der Zeitraum zwischen der Zugabe des flüssigen e) wherein the period between the addition of the liquid
Hydrophobierungsmittels und dem Abschluß des Pressvorganges 60 Minuten nicht übersteigt und  Hydrophobing agent and the completion of the pressing process does not exceed 60 minutes and
f) nachfolgend die in den Hohlkammern des Lochziegels (4) verpresste Mischung, bevorzugt bei einer Temperatur von 20 bis 80 °C, nachreagieren läßt. f) subsequently allowed to react in the hollow chambers of the perforated brick (4) pressed mixture, preferably at a temperature of 20 to 80 ° C.
Die Nummerierung (1 ) - (7) bezieht sich auf Figur 1 . A bedeutet die Bewegung des Pressstempels (5) nach unten, B das beidseitige Pressen der Pressstempel (5) und (6). The numbering (1) - (7) relates to FIG. 1. A means the movement of the ram (5) down, B the two-sided pressing of the ram (5) and (6).
Pyrogene Kieselsäuren werden durch Flammenhydrolyse von Pyrogenic silicas are obtained by flame hydrolysis of
Siliciumverbindungen, wie beispielsweise Chlorsilanen, hergestellt. Bei diesem Verfahren wird ein hydrolysierbares Siliciumhalogenid mit einer Flamme zur Reaktion gebracht, die durch Verbrennung von Wasserstoff und eines Silicon compounds, such as chlorosilanes produced. In this process, a hydrolyzable silicon halide is reacted with a flame formed by combustion of hydrogen and a
sauerstoffhaltigen Gases gebildet worden ist. Die Verbrennungsflamme stellt dabei Wasser für die Hydrolyse des Siliciumhalogenides und genügend Wärme zur Hydrolysereaktion zur Verfügung. Eine so hergestellte Kieselsäure wird als pyrogene Kieselsäure bezeichnet. Bei diesem Prozess werden zunächst Primärpartikel gebildet, die nahezu frei von inneren Poren sind. Diese oxygen-containing gas has been formed. The combustion flame thereby provides water for the hydrolysis of the silicon halide and sufficient heat for the hydrolysis reaction. A silica prepared in this way is called fumed silica. In this process, first Primary particles formed that are almost free of internal pores. These
Primärteilchen verschmelzen während des Prozesses über sogenannte „Sinterhälse" zu dreidimensionalen Aggregaten. Aufgrund dieser Struktur ist pyrogen hergestellte Kieselsäure ein ideales Dämmmaterial, da die Primary particles merge into three-dimensional aggregates during the process via so-called "sintering necks." Due to this structure, fumed silica is an ideal insulating material because of its structure
Aggregatstruktur eine hinreichende mechanische Stabilität bewirkt, die Aggregate structure causes sufficient mechanical stability, the
Wärmeübertragung durch Festkörperleitfähigkeit über die„Sinterhälse" minimiert und eine ausreichend hohe Porosität erzeugt. Bei der eingesetzten pyrogenen Kieselsäure handelt es sich um eine hydrophile Kieselsäure, wie sie im Heat transfer through solid-state conductivity through the "sintered necks" is minimized and a sufficiently high porosity is produced The fumed silica used is a hydrophilic silica, as used in the US Pat
geschilderten Verfahren erhalten wird. Diese Kieselsäure trägt auf ihrer described method is obtained. This silica carries on its
Oberfläche Hydroxylgruppen in Form von Si-OH. Bei den pyrogenen hydrophilen Kieselsäuren beträgt die Silanolgruppendichte in der Regel 1 ,8 bis 2,5, wenn sie durch Reaktion des Siliciumdioxidpulvers mit LiAIH4 nach der Methode von J. Mathias und G. Wannemacher (Journal of Colloid and Interface Science 125, 1988, 61 ) bestimmt wird. Im Unterschied zu einer hydrophoben Kieselsäure soll die Oberfläche der hydrophilen Kieselsäure nicht mit einem organischen oder anorganischen Hydrophobierungsmittel behandelt sein. Surface hydroxyl groups in the form of Si-OH. In the case of fumed hydrophilic silicas, the silanol group density is generally from 1.8 to 2.5 when obtained by reaction of the silica powder with LiAlH 4 according to the method of J. Mathias and G. Wannemacher (Journal of Colloid and Interface Science 125, 1988, 61) is determined. Unlike a hydrophobic silica, the surface of the hydrophilic silica should not be treated with an organic or inorganic hydrophobing agent.
Im Rahmen der Erfindung bedeutet pyrogene Kieselsäure eine pulverförmige, pyrogene, hydrophile Kieselsäure. In the context of the invention, fumed silica means a powdery, fumed, hydrophilic silica.
Die pyrogene Kieselsäure kann auch in verdichteter Form, das heißt mit The fumed silica can also be in a condensed form, ie with
Stampfdichten bestimmt nach DIN EN ISO 787/1 1 von mehr als 80 g/l, in der Regel > 80 bis 150 g/l, eingesetzt werden. Typische Stampfdichten der nicht pyrogenen Kieselsäure betragen 30 bis 60 g/l. Bevorzugt kommen pyrogene Kieselsäuren mit einer BET-Oberfläche von 90 m2/g oder mehr, besonders bevorzugt von 150 bis 500 m2/g zum Einsatz. Puncture densities determined according to DIN EN ISO 787/1 1 of more than 80 g / l, usually> 80 to 150 g / l, are used. Typical tamped densities of the non-fumed silica are 30 to 60 g / l. Preference is given to pyrogens Silicas having a BET surface area of 90 m 2 / g or more, more preferably from 150 to 500 m 2 / g are used.
Bei den im erfindungsgemäßen Verfahren eingesetzten Trübungsmitteln handelt es sich bevorzugt um Titanoxide, Zirkonoxide, llmenite, Eisentitanate, Eisenoxide, Zirkonsilikate, Siliciumcarbid, Manganoxide, Graphite und/oder Ruße, oder um Stoffgemische, welche mindestens einen der vorgenannten Bestandteile umfassen. Besonders bevorzugt handelt es sich um Siliciumcarbid, Titanoxide, Eisenoxide oder Ruße. Die Partikelgröße der Trübungsmittel liegt in der Regel zwischen 0,1 bis 25 μιτι. Bei Siliciumcarbid und Titanoxiden ist der mittlerer Partikeldurchmesser d5o bevorzugt 1 bis 10 μιτι, besonders bevorzugt 2 bis 8 μιτι. The opacifiers used in the process according to the invention are preferably titanium oxides, zirconium oxides, ilmenites, iron titanates, iron oxides, zirconium silicates, silicon carbide, manganese oxides, graphites and / or carbon blacks, or mixtures of substances which comprise at least one of the abovementioned constituents. Particular preference is given to silicon carbide, titanium oxides, iron oxides or carbon blacks. The particle size of the opacifier is usually between 0.1 to 25 μιτι. In the case of silicon carbide and titanium oxides, the mean particle diameter d 5 o is preferably 1 to 10 μm, more preferably 2 to 8 μm.
Zur mechanischen Verstärkung werden zusätzlich Fasern eingesetzt werden. Diese Fasern können anorganischen oder organischen Ursprungs sein. Beispiele einsetzbarer anorganischer Fasern sind Glaswolle, Steinwolle, Basalt-Fasern, Schlacken-Wolle und keramische Fasern, die aus Schmelzen von Aluminiumoxid und/oder Siliciumdioxid, sowie weiteren anorganischen Metalloxiden bestehen. Reine Siliciumdioxidfasern sind beispielsweise Silica-Fasern. Beispiele For mechanical reinforcement additional fibers will be used. These fibers may be of inorganic or organic origin. Examples of usable inorganic fibers are glass wool, rock wool, basalt fibers, slag wool and ceramic fibers, which consist of melts of alumina and / or silica, and other inorganic metal oxides. Pure silica fibers are, for example, silica fibers. Examples
einsetzbarer organischer Fasern sind Cellulosefasern, Textilfasern oder usable organic fibers are cellulose fibers, textile fibers or
Kunststofffasern. Der Durchmesser der Fasern beträgt bevorzugt 1 bis 30 μιτι, besonders bevorzugt 5 bis 15 μιτι, ganz besonders bevorzugt 6 bis 9 μιτι, und die Länge beträgt bevorzugt 1 bis 25 mm, besonders bevorzugt 3 bis 12 mm. Plastic fibers. The diameter of the fibers is preferably 1 to 30 μιτι, more preferably 5 to 15 μιτι, most preferably 6 to 9 μιτι, and the length is preferably 1 to 25 mm, more preferably 3 to 12 mm.
Das im erfindungsgemäßen Verfahren eingesetzte Gemisch (1 ) enthält The mixture used in the process according to the invention (1)
bevorzugt 5 bis 96 Gew.%, besonders bevorzugt 50 bis 92 Gew.% pyrogene Kieselsäure; bevorzugt 3 bis 40 Gew.%, besonders bevorzugt 5 bis 20 Gew.% Trübungsmittel und bevorzugt 1 bis 20 Gew.%, besonders bevorzugt 2 bis 8 Gew.% Fasern. preferably 5 to 96% by weight, particularly preferably 50 to 92% by weight, of fumed silica; preferably 3 to 40% by weight, particularly preferably 5 to 20% by weight Opacifier and preferably 1 to 20 wt.%, Particularly preferably 2 to 8 wt.% Fibers.
Bei dem Hydrophobierungsmittel handelt es sich bevorzugt um ein Organosilan der Summenformel Rn-Si-X4.n, RnSinOn, mit n = 1 -4; R = -H, -CH3, -C2H5; X = -Cl, -Br; -OCH3, -OC2H5, -OC3H8 und/oder Hexamethyldisilazan, (CH3)3SiNHSi(CH3)3. Besonders bevorzugt kann Hexamethyldisilazan eingesetzt werden, da das bei der Hydrophobierungsreaktion entstehende geringe Ammoniakgasvolumen die Entgasung während des Pressvorganges kaum beeinflußt. Der Anteil des The hydrophobizing agent is preferably an organosilane of the empirical formula R n -Si-X 4 . n , R n Si n O n , where n = 1 -4; R = -H, -CH 3 , -C 2 H 5 ; X = -Cl, -Br; -OCH 3 , -OC 2 H 5 , -OC 3 H 8 and / or hexamethyldisilazane, (CH 3 ) 3SiNHSi (CH 3 ) 3. Hexamethyldisilazane can be used with particular preference since the small volume of ammonia gas formed during the hydrophobization reaction hardly influences degassing during the pressing process. The share of
Hydrophobierungsmittels beträgt bevorzugt 0,5 - 10 Gew.%, besonders bevorzugt 1 bis 6 Gew.%, jeweils bezogen auf das Gemisch (1 ). Hydrophobizing agent is preferably 0.5 to 10 wt.%, Particularly preferably 1 to 6 wt.%, Each based on the mixture (1).
Das Hydrophobierungsmittel wird in flüssiger Form, möglichst fein verteilt in das Gemisch (1 ) eingebracht. Dabei befindet sich das Gemisch (1 ) bevorzugt in Bewegung, beispielsweise durch Rühren. Das Hydrophobierungsmittel kann durch eine druckluftfreie Zerstäubung oder durch in das Gemisch (1 ) ragende Kanülen eingebracht werden. The hydrophobing agent is introduced in liquid form, as finely divided as possible into the mixture (1). In this case, the mixture (1) is preferably in motion, for example by stirring. The hydrophobizing agent can be introduced by a compressed air-free atomization or by in the mixture (1) projecting cannulas.
Es ist darauf zu achten, dass das Hydrophobierungmittel rasch in das Gemisch (1 ) eingearbeitet wird. Bevorzugt wird dieser Vorgang in einem Zeitraum von nicht mehr als 5 min, besonders bevorzugt von 10 s bis 3 min und ganz besonders von 30 s bis 90 s durchgeführt. Care must be taken that the hydrophobing agent is rapidly incorporated into the mixture (1). Preferably, this process is carried out in a period of not more than 5 minutes, more preferably from 10 seconds to 3 minutes and most preferably from 30 seconds to 90 seconds.
Der Prozessschritt der Hydrophobierung ist vom Wassergehalt der pyrogenen Kieselsäure abhängig. Der Wassergehalt sollte nicht mehr als 1 Gew.-%, bezogen auf das Gemisch (1 ), betragen. Gegebenenfalls kann das Gemisch (1 ) und/oder der Lochziegel zur Verringerung des Wassergehaltes temperiert dem Prozess zugeführt werden. The process step of the hydrophobing is dependent on the water content of the fumed silica. The water content should not be more than 1% by weight, based on the mixture (1). Optionally, the mixture (1) and / or the perforated brick to reduce the water content tempered to be fed to the process.
Als Lochziegel (4) können sowohl gebrannte Ziegel als auch kaltgeformte Steine, beispielsweise zementgebundene Bimssteine, zur Anwendung kommen. Both perforated bricks and cold-formed bricks, for example cement-bound pumice stones, can be used as perforated bricks (4).
Das erfindungsgemäße Verfahren weist einen Reaktionsschritt auf, bei dem man die verpresste Mischung in den Hohlkammern des Lochziegels (4) nachreagieren läßt. Die Nachreaktion dient im wesentlichen dazu die Hydrophobierung The process according to the invention has a reaction step in which the compressed mixture in the hollow chambers of the perforated brick (4) can be allowed to react. The secondary reaction essentially serves to hydrophobize
vollständig abzuschließen. Eine zu schnelle, d. h. eine bei relativ hohen completely complete. Too fast, d. H. one at a relatively high
Temperaturen vorgenommene Nachreaktion kann dazu führen, dass die gasförmigen Reaktionsprodukte zu heftig austreten und dabei das Gefüge des Dämmstoffes zerstören. Daher hat es sich als vorteilhaft verwiesen, die Temperature post-reaction can cause the gaseous reaction products to escape too vigorously and thereby destroy the structure of the insulating material. Therefore, it has been found advantageous, the
Nachreaktion so auszuführen, dass man ausgehend von 20-30 °C kontinuierlich über einen Zeitraum von 20-90 min, besonders bevorzugt 30-60 min auf eine Temperatur von 50-100 °C erwärmt, und gegebenenfalls bei der höchsten Reaction to be carried out so that, starting from 20-30 ° C continuously heated over a period of 20-90 minutes, more preferably 30-60 minutes to a temperature of 50-100 ° C, and optionally at the highest
Temperatur eine Haltezeit von 10-20 min beibehält. Temperature maintains a holding time of 10-20 min.
Die verpresste Mischung kann mitunter einen sogenannten„spring-back"-Effekt aufweisen, d. h. sie kann sich nach dem Pressen wieder etwas ausdehnen. Dies führt einerseits zur notwendigen Verankerung in der Hohlkammer des Bausteines, andererseits kann ein Teil der verpressten Mischung über die die The compressed mixture can sometimes have a so-called "spring-back" effect, that is, it can expand slightly after pressing, which on the one hand leads to the necessary anchoring in the hollow chamber of the building block, on the other hand, a part of the compressed mixture on the
Lochziegeloberfläche hinausragen, wenn die Verpressung bündig mit der Projecting hole surface when the compression flush with the
Oberfläche stattfindet. Dies kann verhindert werden, wenn geeignet profilierte Pressstempel wenigstens 2 mm, bevorzugt 2 - 5 mm in die die Mischung aufweisende Kammer eintauchen. Die mittlere Dichte der verpressten Mischung beträgt in der Regel 100 bis 150 kg/m3. Surface takes place. This can be prevented if suitably profiled press dies of at least 2 mm, preferably 2 to 5 mm, dip into the chamber having the mixture. The average density of the compressed mixture is usually 100 to 150 kg / m 3 .
Beispiel example
Hochlochziegel: MZ 8 mit 12 Hohlkammern, Ziegelverbund„Mein Ziegelhaus". Hollow brick: MZ 8 with 12 hollow chambers, brick composite "My brick house".
Gemisch (1 ): Es wird ein Gemisch bestehend aus 83 Gew.-% AEROSIL® 200, Evonik, 16 Gew.-% Siliciumcarbid und 1 Gew.-% Fasern eingesetzt. Mixture (1): A mixture consisting of 83% by weight of AEROSIL® 200, Evonik, 16% by weight of silicon carbide and 1% by weight of fibers is used.
Als Hydrophobierungsmittel dient Hexamethyldisilazan, 4 Gew.-% bezogen auf das Gemisch (1 ). The hydrophobizing agent used is hexamethyldisilazane, 4% by weight, based on the mixture (1).
Der Mischvorgang wird in einem geschlossenen Behälter unter Verwendung eines Rühraggregates bei einer Umdrehungsgeschwindigkeit von 1000 - 1500 UpM durchgeführt. Die Rührzeit beträgt ca. 30 - 60 s, in dieser Zeit wird in den ersten 30 - 45 s das Hydrophobierungsmittel eingespritzt und anschließend noch ca. 15 s weiter gerührt. Die Temperatur beträgt ca. 20 °C an. Die Mischung wird in die obere Füllröhre (2) gefördert. Der untere Pressstempel (5) fährt nach unten (A) und saugt die Mischung durch die Hohlkammer des Lochziegels (4) in die untere Füllröhre (3). Die Verdichtung der Mischung erfolgt beim Pressen gleichzeitig und beidseitig 2 - 3 mm in den Lochziegel hinein. Unmittelbar vor der Pressphase und während des Pressvorgangs wird die überschüssige Luft über Filterplatten durch die Pressstempel abgesaugt (7). The mixing operation is carried out in a closed container using a stirrer at a rotation speed of 1000 - 1500 rpm. The stirring time is approx. 30 - 60 s, during which time the water repellent is injected for the first 30 - 45 s and then stirred for a further 15 s. The temperature is about 20 ° C on. The mixture is conveyed into the upper filling tube (2). The lower ram (5) moves downwards (A) and sucks the mixture through the hollow chamber of the perforated brick (4) into the lower filling tube (3). The compaction of the mixture takes place during pressing at the same time and on both sides 2 - 3 mm into the perforated brick. Immediately before the pressing phase and during the pressing process, the excess air is sucked through filter plates through the press punches (7).
Der Pressvorgang ist innerhalb ca. 10 min beendet. Nachfolgend wird über einen Zeitraum von 50 min die Temperatur auf 60 °C gesteigert und dort für 10 min belassen. Nach ca. 30 - 45 min bei einer Temperatur von ca. 60 °C ist die Reaktion im Lochziegel abgeschlossen, die Wärmedämmstoffmischung durchgehend hydrophobiert und die Entgasung weitgehend erfolgt. The pressing process is completed within 10 minutes. Subsequently, the temperature is increased to 60 ° C over a period of 50 min and left there for 10 min. After about 30 - 45 minutes at a temperature of about 60 ° C is the Completed reaction in the perforated brick, the thermal insulation mixture continuously hydrophobic and the degassing occurs largely.
Beim erhaltenen Lochziegel ist keine Hydrophobierung der Bausteinoberflächen festzustellen. Der Ziegelscherben ist auch in unmittelbarer Nähe der In the obtained perforated brick no hydrophobization of the building blocks surfaces is observed. The Ziegelscherben is also in the immediate vicinity of
hydrophobierten Dämmstoffmischung mit Wasser benetzbar. hydrophobized insulation mixture wetted with water.

Claims

Patentansprüche claims
1 . Verfahren zur Befüllung der Hohlkammern von Lochziegeln mit einer 1 . Method for filling the hollow chambers of perforated bricks with a
Wärmedämmstoffmischung, dadurch gekennzeichnet, dass man  Thermal insulation mixture, characterized in that one
a) ein Gemisch (1 ) das erhalten wird, indem man eine pulverförmige,  a) a mixture (1) which is obtained by mixing a pulverulent,
pyrogene, hydrophile Kieselsäure, pulverförmiges Trübungsmittel und Fasern, bei Temperaturen von weniger als 30 °C mit einem flüssigen Hydrophobierungsmittel versetzt, in eine obere Füllröhre (2) fördert, b) nachfolgend den unteren Pressstempel (5) nach unten bewegt und so einen Teil der sich in der oberen Füllröhre (2) befindlichen Mischung durch die Hohlkammern des Lochziegels (4) in die untere Füllröhre (3) saugt, so dass sich die Mischung in die obere Füllröhre (2), die Hohlkammern des  fumed, hydrophilic silica, powdered opacifier and fibers, at temperatures of less than 30 ° C with a liquid hydrophobing agent, promotes in an upper filling tube (2), b) subsequently moves the lower ram (5) down and so a part of in the upper filling tube (2) located mixture through the hollow chambers of the perforated brick (4) in the lower filling tube (3) sucks, so that the mixture in the upper Füllröhre (2), the hollow chambers of
Lochziegels (4) und in die untere Füllröhre (3) verteilt.  Hollow brick (4) and distributed in the lower filler tube (3).
c) nachfolgend durch beidseitiges Pressen der Pressstempel (5) und (6) die Mischung verdichtet,  c) subsequently compacting the mixture by pressing the press dies (5) and (6) on both sides,
d) wobei vor und während des Pressvorganges gasförmige und  d) wherein before and during the pressing process gaseous and
gegebenenfalls dampfförmige Stoffe über Filterplatten (7) an den  optionally vaporous substances via filter plates (7) to the
Pressstempeln (5) und (6) entfernt wird und  Press punches (5) and (6) is removed and
e) wobei der Zeitraum zwischen der Zugabe des flüssigen  e) wherein the period between the addition of the liquid
Hydrophobierungsmittels und dem Abschluß des Pressvorganges 60 Minuten nicht übersteigt und  Hydrophobing agent and the completion of the pressing process does not exceed 60 minutes and
f) nachfolgend die in den Hohlkammern des Lochziegels (4) verpresste  f) subsequently pressed in the hollow chambers of the perforated brick (4)
Mischung, bevorzugt bei einer Temperatur von 20 bis 100°C, nachreagieren läßt. Mixture, preferably at a temperature of 20 to 100 ° C, allowed to react.
2. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass 2. The method according to claim 1, characterized in that
das Gemisch (1 ) 5 bis 96 Gew.% pyrogene, hydrophile Kieselsäure, 3 bis 40 Gew.% Trübungsmittel und 1 bis 20 Gew.% Fasern enthält.  the mixture (1) contains 5 to 96% by weight of pyrogenic, hydrophilic silica, 3 to 40% by weight of opacifier and 1 to 20% by weight of fibers.
3. Verfahren nach den Ansprüchen 1 oder 2, dadurch gekennzeichnet, dass das Hydrophobierungsmittel ein Organosilan der Summenformel 3. Process according to claims 1 or 2, characterized in that the hydrophobizing agent is an organosilane of the empirical formula
Rn-Si-X4-n, RnSinOn mit n = 1 -4; R = -H, -CH3, -C2H5; X = -Cl, -Br; -OCH3, -OC2H5, -OC3H8 und/oder (CH3)3SiNHSi(CH3)3. ist, Rn-Si-X 4 - n, RnSinOn with n = 1 -4; R = -H, -CH 3 , -C 2 H 5 ; X = -Cl, -Br; -OCH 3 , -OC 2 H 5, -OC 3 H 8 and / or (CH 3 ) 3 SiNHSi (CH 3 ) 3. is
4. Verfahren nach den Ansprüchen 1 bis 3, dadurch gekennzeichnet, dass 4. Process according to claims 1 to 3, characterized in that
der Anteil des Hydrophobierungsmittels 0,5 - 10 Gew.%, bezogen auf das Gemisch (1 ), beträgt.  the proportion of the hydrophobizing agent is 0.5-10% by weight, based on the mixture (1).
5. Verfahren nach den Ansprüchen 1 bis 4, dadurch gekennzeichnet, dass 5. Process according to claims 1 to 4, characterized in that
der Wassergehalt des Gemisches (1 ) und/oder des Lochziegels (4) jeweils höchstens 1 Gew.-% ist.  the water content of the mixture (1) and / or the perforated brick (4) is in each case at most 1% by weight.
6. Verfahren nach den Ansprüchen 1 bis 5, dadurch gekennzeichnet, dass 6. Process according to claims 1 to 5, characterized in that
man die verpresste Mischung in den Hohlkammern des Lochziegels (4) so nachreagieren läßt, dass man diese ausgehend von 20-30°C kontinuierlich über einen Zeitraum von 20-90 min auf eine Temperatur von 50-100 °C erwärmt.  It is possible to react the pressed mixture in the hollow chambers of the perforated brick (4) so that they are heated continuously from 20-30 ° C over a period of 20-90 minutes to a temperature of 50-100 ° C.
7. Verfahren nach den Ansprüchen 1 bis 6, dadurch gekennzeichnet, dass geeignet profilierte Pressstempel wenigstens 2 mm in die die Mischung aufweisende Kammer eintauchen. 7. Process according to claims 1 to 6, characterized in that suitably profiled press punches dive at least 2 mm into the chamber having the mixture.
PCT/EP2014/062816 2013-07-16 2014-06-18 Method for filling cavities in hollow bricks with a thermal insulation material mixture containing a hydrophobing agent WO2015007450A1 (en)

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